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提出了低于GeCl4挥发温度密闭消解AuGe2合金的新技术,研究了微波密闭消解和微波密闭消化罐室温溶解样品的条件,以及水合肼室温还原Au(Ⅲ)为Au(0)和电感耦合等离子体发射光谱法测定Ge的条件。结果表明:当功率600 W,温度70～80℃,压力3238～3652 kPa,升温5 min,恒温1～2 h或室温4～6 h时,9 mL HCl-3 mL H2O2能完全消解或室温溶解0.10 g样品,且Ge无损失。于约15%HCl介质中,水合肼室温能完全还原Au(Ⅲ)为Au(0)。当分析波长为209.426nm时,测定AuGe2合金中Ge的相对标准偏差0.882%和0.833%,样品加标回收率99.32%～100.71%,检出限0.0049μg/mL和线性范围1～506μg/mL。方法结果准确、分析快速、操作简便,已用于实际的样品分析,结果满意。
A new technique of aseptic digestion of AuGe2 alloy below the GeCl4 volatilization temperature was proposed. The conditions of microwave digestion and microwave digestion tank were investigated. The results showed that Au (Ⅲ) was Au (0) and inductively coupled plasma Determination of Ge by Emission Spectrometry. The results showed that 9 mL HCl-3 mL H2O2 could be completely digested or dissolved at room temperature under the conditions of power of 600 W, temperature of 70-80 ℃, pressure of 3238-3652 kPa, temperature of 5 min, constant temperature of 1 ~ 2 h or room temperature of 4 ~ 0.10 g sample without loss of Ge. In about 15% HCl medium, hydrazine hydrate completely reduced Au (Ⅲ) to Au (0) at room temperature. When the analysis wavelength is 209.426nm, the relative standard deviations (RSDs) of Ge in AuGe2 alloy are 0.882% and 0.833%, respectively. The spiked recoveries are 99.32% ~ 100.71%. The detection limits are 0.0049μg / mL and linear range is 1 ~ 506μg / mL. The method is accurate, fast and easy to operate. It has been used in practical sample analysis with satisfactory results.